참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | 2-nitromethylenetetrahydro-2H-1,3-thiazine | HCID 42853 | — |
| 반응물 | Dodecylsulfonyl chloride | HCID 66280 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 3-(Dodecane-1-sulfonyl)-2-(nitromethylidene)-1,3-thiazinane | HCID 53912032 | — |
반응 단계
1.6 g of 2-(nitromethylene)-tetrahydro-2H-1,3-thiazine, 3.18 g of ethyldiisopropylamine and 20 ml of methylene chloride were mixed. The mixture was cooled to and stirred at -60° C. under a nitrogen atmosphere while 2.95 g of dodecanesulfonyl chloride was added in portions over a 10 minute period. The mixture was allowed to warm to 10° C. (2.5 hours), then stirred at 10° C. for 1 hour and at 20° C. for 1.5 hours. The resulting mixture was poured into water, and the organic phase was separated, dried (MgSO4), filtered and stripped of solvent. The residue, a gum, was chromatographed over silica gel, using methylene chloride as eluent. After workup the product was recrystallized from ethanol to give N-(dodecylsulfonyl)-2-(nitromethylene)-tetrahydro-2H-1,3-thiazine (3A) as a solid, m.p.: 116°-117° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04486427 |
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| 출처 데이터셋 | uspto-grants-1984_12 |
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| ORD ID | ord-b1afed8fd099419786edb1cc6b2f27d9 |
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| 출처 메모 | uspto-grants-1984_12 |
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